CN101805146A - Polycarboxylic acid water reducer and preparation method thereof - Google Patents
Polycarboxylic acid water reducer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polycarboxylic acid water reducer and a preparation method thereof. The method for preparing the polycarboxylic acid water reducer comprises the following steps: (1) respectively dropwise adding initiator aqueous solution and monomer mixed aqueous solution consisting of polyethylene glycol (methyl) acrylate monomer, (methyl) acrylic acid monomer, (methyl) acrylate monomer or (methyl) sodium allylsulfonate continuously into a reactor to perform a polymerization reaction, finishing dropwise adding in 2 to 6 hours, and keeping on heat reservation and reaction for 1 to 4 hours; (2) cooling the solution, and adjusting pH value of the solution to be between 6.0 and 8.0 after the reaction is completed, and controlling the mass concentration of the solution to be between 18 and 25 percent. The polycarboxylic acid water reducer has the advantages of high dispersion, strong slump retaining capability, low air-entraining performance, clear intensifying effect, high shrinkage resistance, good viscosity reducing performance and the like, represents excellent comprehensive performance, and has wide application range.
Description
Technical field
The present invention relates to a kind of concrete, mortar poly carboxylic acid series water reducer, be specifically related to a kind of preparation method of poly carboxylic acid series water reducer of high comprehensive performance.
Background technology
Poly carboxylic acid series water reducer is the polymeric surface active agent that the molecule structure contains the carboxyl graft copolymer, have that volume is low, dispersive ability is strong, disperse to keep performance good, produce and use series of advantages such as environmentally safe, obtain the generally approval of concrete works circle for this reason; Simultaneously, because of the plasticity-of its molecular structure is big, product category emerges in an endless stream, and causes the numerous scientific research personnel's of different field research interest, becomes the prime mover that the poly carboxylic acid series water reducer series product are weeded out the old and bring forth the new.At present, the research and development of poly carboxylic acid series water reducer are still the focus of concrete admixture industry research.At home, the research of poly carboxylic acid series water reducer has in recent years obtained very fast development, but compares with external product, many homemade poly carboxylic acid series water reducer The comprehensive performance are obviously relatively poor, be mainly reflected in: bleed is strong excessively, and loss of strength is big, and the 28d compressive strength rate is lower than 100%; Guarantor's ability of collapsing is strong inadequately; A little less than the anti-drying shrinkage ability, 28d contract with dry rate ratio is greater than 100%; Viscosity-reducing performance is poor, and the cement slurry apparent viscosity is big; Quality product is stable inadequately etc.; These all are bottlenecks that homemade poly carboxylic acid series water reducer product need be broken through.
Patent CN 101376576A discloses a kind of prescription and manufacture method thereof of early strength type polycarboxylic acid series high-performance dehydragent, this technology synthetic water reducer has improved epistasis energy morning of poly carboxylic acid series water reducer to a certain extent, but owing to use the allyl polyether monomer, the dispersiveness of water reducer is lower.
Patent CN 101205128A discloses a kind of high-early strength type polycarboxylic acids dehydragent and preparation technology thereof, by in molecular structure, introducing the bleed that the functional group with their defoaming function reduces poly carboxylic acid series water reducer, to improve its early strength function, early potent fruit is better for the water reducer of this technology preparation.
Patent CN 101289292A discloses a kind of early strength polycarboxylic acid high performance dehydragent and preparation method thereof, by accelerating components such as composite trolamine, nitrocalcite and Sodium Thiocyanate 99 in the acrylic acid or the like poly carboxylic acid series water reducer, to improve epistasis energy morning of polycarboxylate water-reducer, effect is better, but the shrinkage ratio of water reducer is bigger, and anti-drying shrinkage ability is relatively poor.
Patent CN 101182156A discloses a kind of decrement reinforcing type polycarboxylic acid series high-performance dehydragent and preparation method thereof, by in molecular structure, introducing the effect of reducing that the functional group with reducing function realizes poly carboxylic acid series water reducer, it is obvious that the poly carboxylic acid series water reducer of this technology preparation reduces effect, but the water reducer volume is bigger, and water-reducing rate is lower.
Comprehensive present disclosed patent documentation, the contriver mainly concentrates on the partial properties that improves poly carboxylic acid series water reducer, and less at the patent documentation that improves the poly carboxylic acid series water reducer over-all properties.The raising of over-all properties to strengthening the poly carboxylic acid series water reducer competitiveness of product in market, enlarging the consistency of its range of application, improvement and cement, has positive pushing effect.
Summary of the invention
The objective of the invention is to overcome the shortcomings and deficiencies of prior art, poly carboxylic acid series water reducer of a kind of high comprehensive performance and preparation method thereof is provided.
Purpose of the present invention is achieved through the following technical solutions:
The molecular structure of poly carboxylic acid series water reducer is shown in general formula (1):
Wherein, R
1, R
2And R
3Identical or different, and represent H or CH separately
3
R
4Expression COOR or CH
2SO
3Na, and R represents the alkyl of 1～4 carbon atom;
M represents H or Na;
M represents the average addition mole number of oxyethylene group, is 1～100 numeral;
A, b, c represent the average number of repeat unit of each monomer in molecular structure;
N represents the mean polymerisation degree of poly carboxylic acid series water reducer molecular structure.
The value of described a, b, c can be respectively: a=20～80, b=3～6, c=20～30; The value of n is 40～120.
Above-mentioned poly carboxylic acid series water reducer, its weight-average molecular weight are 8000～100000.
The preparation method of above-mentioned poly carboxylic acid series water reducer comprises the steps:
(1) monomer mixed aqueous solution and initiator solution are added dropwise to respectively continuously carry out polyreaction in the reactor, in 2～6h, drip off, continue insulation reaction 1～4h afterwards; Except that comprising poly glycol monomethyl ether (methyl) acrylate monomer and (methyl) Acrylic Acid Monomer, also comprise (methyl) acrylic ester monomer or (methyl) sodium allylsulfonate monomer in the described monomer mixed aqueous solution;
(2) reaction finishes, cooling, and regulator solution pH value is 6.0～8.0, solution quality concentration is controlled at 18～25%.
Above-mentioned preparation method, each monomeric molar percentage consists of in the monomer mixed aqueous solution:
Poly glycol monomethyl ether (methyl) acrylate monomer 10～40%;
(methyl) Acrylic Acid Monomer 40～80%;
(methyl) acrylic ester monomer or (methyl) sodium allylsulfonate monomer 2～20%.
Among the above-mentioned preparation method, described initiator is one or both in persulphate, the hydrogen peroxide.
Among the above-mentioned preparation method, described initiator amount is 1～15% of a monomer total mass.
Evaluation for over-all properties, draw through for many years practice, excellent several salient features (dispersing propertys of poly carboxylic acid series water reducer product requirement, disperse to keep performance, the bleed performance, epistasis energy early, anti-shrinkage performance, viscosity-reducing performance etc.) in same types of molecules structure and same parent, obtain organically unified (or compatible), be that above-mentioned several salient features can reach higher level simultaneously, this need realize that with the control molecular structure prerequisite is that the theory of molecular structure and property relationship is innovated and deep understanding to some extent by the relation and the more rational design of more deep research molecular structure and performance.
Compare with existing public technology, the present invention has tangible novelty and advantage, is specifically described as follows:
(1) the present invention controls its bleed performance, anti-shrinkage performance and viscosity-reducing performance by the molecular structure of optimizing poly carboxylic acid series water reducer under the condition of not adding defoamer and economization agent, has novelty;
(2) although the present invention not in molecular structure grafting have the functional group of their defoaming function, reducing function, prepared poly carboxylic acid series water reducer have a strong advantage of low, the anti-drying shrinkage ability of bleed;
(3) poly carboxylic acid series water reducer of the present invention preparation, advantage such as it is good to have a dispersing property, and it is strong to protect the ability of collapsing, and bleed is low, reinforced effects is obvious, anti-drying shrinkage ability is strong, viscosity-reducing performance is good shows excellent comprehensive performances, and applied widely, the market competitiveness is strong.
Embodiment
The invention will be further described below in conjunction with embodiment, enumerates the part specific embodiment below, but the scope of protection of present invention is not limited to the scope of embodiment statement.
In an embodiment, except as otherwise noted, otherwise " % " expression " quality % ".
In an embodiment, weight-average molecular weight is the weight-average molecular weight of employing gel permeation chromatography (GPC) mensuration, and represents based on the equivalent of polyoxyethylene glycol.
Synthetic embodiment 1
With polyethylene glycol monomethyl ethermethacrylic acid esters (the average addition mole number of ethylene oxide is 22) 30g, methacrylic acid 5.596g, methyl methacrylate 0.501g and deionized water, be made into concentration and be 70% the mix monomer aqueous solution, standby; With concentration be 30% hydrogen peroxide 4.813g and deionized water to be made into concentration be 2.1% initiator solution, standby.
In the glass reactor of being furnished with thermometer, agitator, reflux condensing tube, dropper, nitrogen gatherer (capacity is 500ml), add deionized water 30g, stirring heating, letting nitrogen in and deoxidizing simultaneously.When being warming up to 75～85 ℃, begin simultaneously to drip the mix monomer aqueous solution and initiator solution, all in 4.3h, drip off, afterwards insulation reaction 2.7h.Reaction finishes, and is cooled to room temperature, is that the pH value of 30% sodium hydrate regulator solution is 6.0～8.0 with concentration, and is 18.8% with deionized water regulator solution solids content.The gained brown-red solution is poly carboxylic acid series water reducer PCWR-1 of the present invention, and weight-average molecular weight is 42000.Concrete molecular formula is as follows:
R
4Expression COOR, R represents the alkyl of 1～4 carbon atom, M represents Na.
Synthetic embodiment 2
With polyethylene glycol monomethyl ethermethacrylic acid esters (the average addition mole number of ethylene oxide is 22) 30g, methacrylic acid 5.596g, methyl methacrylate 0.501g and deionized water, be made into concentration and be 70% the mix monomer aqueous solution, standby; Being made into concentration with ammonium persulphate 1.444g and deionized water is 2.5% initiator solution, standby.
In the glass reactor of being furnished with thermometer, agitator, reflux condensing tube, dropper, nitrogen gatherer (capacity is 500ml), add deionized water 30g, stirring heating, letting nitrogen in and deoxidizing simultaneously.When being warming up to 75～85 ℃, begin simultaneously to drip the mix monomer aqueous solution and initiator solution, all in 4h, drip off, afterwards insulation reaction 3h.Reaction finishes, and is cooled to room temperature, is that the pH value of 30% sodium hydrate regulator solution is 6.0～8.0 with concentration, and is 19.4% with deionized water regulator solution solids content.The gained yellow solution is poly carboxylic acid series water reducer PCWR-2 of the present invention, and weight-average molecular weight is 69700.Concrete molecular formula is as follows:
R
4Expression COOR, R represents the alkyl of 1～4 carbon atom, M represents Na.
Synthetic embodiment 3
With polyethylene glycol monomethyl ethermethacrylic acid esters (the average addition mole number of ethylene oxide is 22) 45g, methacrylic acid 8.394g, methyl methacrylate 0.751g and deionized water are made into concentration and are 70% the mix monomer aqueous solution, and be standby; Being made into concentration with ammonium persulphate 1.624g and deionized water is 2.1% initiator solution, standby.
In the glass reactor of being furnished with thermometer, agitator, reflux condensing tube, dropper, nitrogen gatherer (capacity is 500ml), add deionized water 30g, stirring heating, letting nitrogen in and deoxidizing simultaneously.When being warming up to 75～85 ℃, begin to drip the mix monomer aqueous solution and initiator solution simultaneously, in 4.4h and 4.5h, drip off respectively, afterwards insulation reaction 2.5h.Reaction finishes, and is cooled to room temperature, is that the pH value of 30% sodium hydrate regulator solution is 6.0～8.0 with concentration, and is 24.3% with deionized water regulator solution solids content.The gained yellow solution is poly carboxylic acid series water reducer PCWR-3 of the present invention, and weight-average molecular weight is 35000.Concrete molecular formula is as follows:
R
4Expression COOR, R represents the alkyl of 1～4 carbon atom, M represents Na.
Synthetic embodiment 4
With polyethylene glycol monomethyl ethermethacrylic acid esters (the average addition mole number of ethylene oxide is 22) 45g, methacrylic acid 8.394g, methyl methacrylate 0.751g and deionized water are made into concentration and are 70% the mix monomer aqueous solution, and be standby; Being made into concentration with ammonium persulphate 1.083g and deionized water is 1.4% initiator solution, standby.
In the glass reactor of being furnished with thermometer, agitator, reflux condensing tube, dropper, nitrogen gatherer (capacity is 500ml), add deionized water 30g, stirring heating, letting nitrogen in and deoxidizing simultaneously.When being warming up to 75～85 ℃, begin to drip the mix monomer aqueous solution and initiator solution simultaneously, in 4.8h and 4.9h, drip off respectively, afterwards insulation reaction 2.1h.Reaction finishes, and is cooled to room temperature, is that the pH value of 30% sodium hydrate regulator solution is 6.0～8.0 with concentration, and is 24.4% with deionized water regulator solution solids content.The gained yellow solution is poly carboxylic acid series water reducer PCWR-4 of the present invention, and weight-average molecular weight is 35100.Concrete molecular formula is as follows:
R
4Expression COOR, R represents the alkyl of 1～4 carbon atom, M represents Na.
Synthetic embodiment 5
With polyethylene glycol monomethyl ethermethacrylic acid esters (the average addition mole number of ethylene oxide is 22) 30g, methacrylic acid 8.179g, methylpropene sodium sulfonate 1.582g and deionized water are made into concentration and are 70% the mix monomer aqueous solution, and be standby; Being made into concentration with Potassium Persulphate 0.795g, 30% hydrogen peroxide 2.65g and deionized water is 2.8% initiator solution, standby.
In the glass reactor of being furnished with thermometer, agitator, reflux condensing tube, dropper, nitrogen gatherer (capacity is 500ml), add deionized water 30g, stirring heating, letting nitrogen in and deoxidizing simultaneously.When being warming up to 75～85 ℃, begin to drip the mix monomer aqueous solution and initiator solution simultaneously, in 4.2h and 4.3h, drip off respectively, afterwards insulation reaction 2.7h.Reaction finishes, and is cooled to room temperature, is that the pH value of 30% sodium hydrate regulator solution is 6.0～8.0 with concentration, and is 19.6% with deionized water regulator solution solids content.The gained yellow solution is poly carboxylic acid series water reducer PCWR-5 of the present invention, and weight-average molecular weight is 17400.Concrete molecular formula is as follows:
R
4Expression CH
2SO
3Na, M represents Na.
Synthetic embodiment 6
With polyethylene glycol monomethyl ethermethacrylic acid esters (the average addition mole number of ethylene oxide is 22) 30g, methacrylic acid 8.179g, methylpropene sodium sulfonate 1.582g and deionized water are made into concentration and are 70% the mix monomer aqueous solution, and be standby; Being made into concentration with Potassium Persulphate 1.193g and deionized water is 2.0% initiator solution, standby.
In the glass reactor of being furnished with thermometer, agitator, reflux condensing tube, dropper, nitrogen gatherer (capacity is 500ml), add deionized water 30g, stirring heating, letting nitrogen in and deoxidizing simultaneously.When being warming up to 75～85 ℃, begin to drip the mix monomer aqueous solution and initiator solution simultaneously, in 4.7h and 4.9h, drip off respectively, afterwards insulation reaction 2.1h.Reaction finishes, and is cooled to room temperature, is that the pH value of 30% sodium hydrate regulator solution is 6.0～8.0 with concentration, and is 19.9% with deionized water regulator solution solids content.The gained yellow solution is poly carboxylic acid series water reducer PCWR-6 of the present invention, and weight-average molecular weight is 16400.
R
4Expression CH
2SO
3Na, M represents Na.
Application Example
The performance of the poly carboxylic acid series water reducer that is obtained among the synthetic embodiment under clean slurry and mortar distinguished as shown in Table 1 and Table 2, and used cement is Guangdong show board P.II 42.5R silicate cement.
The test of clean slurry degree of mobilization is carried out according to standard GB/T 8077-2000, with the size of Marsh-Cone time representation slurry viscosity and through the time change.
Ultimate compression strength, air content and water-reducing rate test require to carry out according to standard GB/T17671-1999 with the preparation of mortar, and the maintenance degree of mobilization is 180 ± 5mm.The method of the constant mortar examination body of fixedly Water Usage Per Unit Volume and slurry volume content standard sand consumption is adopted in contract with dry rate test, and testing method is carried out according to industry standard JC/T 603-2004 requirement.
The Application Example presentation of results, the poly carboxylic acid series water reducer of the present invention's preparation shows excellent comprehensive performances, has advantages such as bleed is low, reinforced effects is obvious, anti-drying shrinkage ability is strong, viscosity-reducing performance is good.
Table 1
Table 2
Claims (8)
1. poly carboxylic acid series water reducer, its molecular structure is shown in general formula (1):
Wherein, R
1, R
2And R
3Identical or different, and represent H or CH separately
3
R
4Expression COOR or CH
2SO
3Na, and R represents the alkyl of 1～4 carbon atom;
M represents H or Na;
M represents the average addition mole number of oxyethylene group, is 1～100 numeral;
A, b, c represent the average number of repeat unit of each monomer in molecular structure;
N represents the mean polymerisation degree of poly carboxylic acid series water reducer molecular structure.
2. poly carboxylic acid series water reducer according to claim 1 is characterized in that the value of described a, b, c is respectively: a=30～120, b=3～6, c=20～30; The value of n is 40～200.
3. poly carboxylic acid series water reducer according to claim 1 is characterized in that its weight-average molecular weight is 8000～50000.
4. the preparation method of the described poly carboxylic acid series water reducer of claim 1 is characterized in that comprising the steps:
(1) monomer mixed aqueous solution and initiator solution are added dropwise to respectively continuously carry out polyreaction in the reactor, in 2～6h, drip off, continue insulation reaction 1～4h afterwards; Except that comprising poly glycol monomethyl ether (methyl) acrylate monomer and (methyl) Acrylic Acid Monomer, also comprise (methyl) acrylic ester monomer or (methyl) sodium allylsulfonate monomer in the described monomer mixed aqueous solution;
(2) reaction finishes, cooling, and regulator solution pH value is 6.0～8.0, solution quality concentration is controlled at 18～25%.
5. preparation method according to claim 4 is characterized in that, each monomeric molar percentage consists of in the monomer mixed aqueous solution:
Poly glycol monomethyl ether (methyl) acrylate monomer 10～40%;
(methyl) Acrylic Acid Monomer 40～80%;
(methyl) acrylic ester monomer or (methyl) sodium allylsulfonate monomer 2～20%.
6. preparation method according to claim 5 is characterized in that, described initiator is one or both in persulphate, the hydrogen peroxide.
7. according to each described preparation method of claim 4～6, it is characterized in that described initiator amount is 1～15% of a monomer total mass.
8. preparation method according to claim 7, it is characterized in that step (1) is carried out also being included in the described reactor before the polyreaction and added deionized water, stirring heating, when being warming up to 75～85 ℃, begin to drip described monomer mixed aqueous solution and initiator solution.
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| CN102532435A (en) * | 2011-12-21 | 2012-07-04 | 湖北恒利建材科技有限公司 | Polycarboxylene high-performance water reducing agent and preparation method thereof |
| CN103011660A (en) * | 2012-12-21 | 2013-04-03 | 江西迪特科技有限公司 | Method for preparing concrete water reducing agent, method for preparing concrete early strength agent through water reducing agent and construction method for concrete early strength agent |
| CN104591583A (en) * | 2015-02-05 | 2015-05-06 | 江苏苏博特新材料股份有限公司 | Anti-cracking additive for concrete |
| CN105461866A (en) * | 2014-09-05 | 2016-04-06 | 深圳市迈地砼外加剂有限公司 | Viscosity-reducing type polycarboxylic-acid water-reducing agent and preparation method thereof |
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| CN102532435B (en) * | 2011-12-21 | 2013-10-30 | 湖北恒利建材科技有限公司 | Polycarboxylene high-performance water reducing agent and preparation method thereof |
| CN102532435A (en) * | 2011-12-21 | 2012-07-04 | 湖北恒利建材科技有限公司 | Polycarboxylene high-performance water reducing agent and preparation method thereof |
| CN103011660A (en) * | 2012-12-21 | 2013-04-03 | 江西迪特科技有限公司 | Method for preparing concrete water reducing agent, method for preparing concrete early strength agent through water reducing agent and construction method for concrete early strength agent |
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| CN105461866B (en) * | 2014-09-05 | 2018-04-06 | 深圳市迈地砼外加剂有限公司 | A kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof |
| CN104591583A (en) * | 2015-02-05 | 2015-05-06 | 江苏苏博特新材料股份有限公司 | Anti-cracking additive for concrete |
| CN105732911B (en) * | 2016-01-15 | 2018-02-23 | 江苏苏博特新材料股份有限公司 | The preparation method and application of viscosity reduction type polycarboxylate water-reducer |
| CN105732911A (en) * | 2016-01-15 | 2016-07-06 | 江苏苏博特新材料股份有限公司 | Preparation method and application of viscosity-reducing polycarboxylate superplasticizer |
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| CN106749963B (en) * | 2016-11-29 | 2019-11-26 | 中建商品混凝土（福建）有限公司 | A kind of bleed controllable type poly carboxylic acid series water reducer and preparation method thereof for pure machine-made sand concrete |
| CN106632889A (en) * | 2016-12-27 | 2017-05-10 | 陕西友邦新材料科技有限公司 | Low air-entrained and viscosity-reduced slow-release polycarboxylate water reducer and preparation method thereof |
| CN106967200A (en) * | 2017-03-31 | 2017-07-21 | 刘翠芬 | It is a kind of to have poly carboxylic acid series water reducer that guarantor is collapsed with viscosity-reducing performance and preparation method thereof concurrently |
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| CN108409919B (en) * | 2018-03-21 | 2021-02-05 | 厦门路桥翔通建材科技有限公司 | Nanoparticle type polycarboxylate superplasticizer and preparation method thereof |
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Application publication date: 20100818 |